CN101462867A - Method for preparing BeO ceramic by gel injection moulding forming technique - Google Patents
Method for preparing BeO ceramic by gel injection moulding forming technique Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramics, in particular relates to a method for preparing BeO ceramics by gel-casting technology. The method comprises the following steps: BeO powder pre-processing, batching, ball milling and material mixing, vacuum degassing, gel curing, drying and gel removal, and sintering. The method for preparing the BeO ceramics has the advantages of simple processing of raw materials, short process, low equipment investment and low cost; and the method helps reduce the contact of an operator with the BeO powder and lower the poison of the BeO, and is suitable for industrialized mass production.
Description
Technical field
The invention belongs to the ceramic technology field, be specifically related to a kind of method of utilizing the gel casting forming technology to prepare the BeO pottery.
Background technology
Beryllium oxide ceramics (BeO) has high heat conductance, high-melting-point, high strength, high-insulativity, high chemistry and thermostability, low-k, low dielectric loss and good characteristics such as Technological adaptability because of it, is used widely in extraordinary metallurgy, vacuum electronic technology, nuclear technique, microelectronics and photoelectron technology field.
The forming method of BeO pottery mainly contains: compression molding, roll [beryllium oxide, metallurgical industry press, 2006] such as embrane method and doctor-blade casting processes, but all there is different shortcomings in the whole bag of tricks.Though the compression molding less investment, production efficiency is low; Roll in the base substrate that embrane method obtains and have anisotropic problem; Doctor-blade casting process must have special-purpose production unit, costs an arm and a leg, and is unfavorable for scale operation etc.The present invention proposes to adopt that a kind of novel forming process of ceramics technology---the gel casting forming technology prepares the BeO pottery.
The gel casting forming technology is a kind of new forming process of ceramics technology [the US Patent that the beginning of the nineties in last century, people such as U.S.'s Oak Ridge professor MarkA.Janney of National Key Laboratory proposed, 5145908,1992], it combines traditional ceramics technology and polymer chemistry first, has started the technology of utilizing the high polymer monomer polymerization to carry out moulding in ceramic molding.This method at first is scattered in ceramic powder in the aqueous solution that contains organic monomer and linking agent, prepare the concentrated suspension of low viscosity and high solid volume fraction, add initiator then, suspensoid is injected mould, at certain temperature or adding catalyzer, cause the organic monomer polymerization, suspensoid viscosity increases severely, cause consolidation in-situ forming, obtain the very high base substrate of intensity through cryodrying.Since occurring the nineties in last century, this moulding process is once the very big attention that proposes just to be subjected to domestic and international research department and industry member, and developed countries such as the U.S. and Japan have listed it in the development and the research project of ceramic new material.
In more than ten years, the development of gel casting forming technology is very rapid in the past, mainly studies and application concentrates on Al
2O
3, SiC, Si
3N
4, ZrO
2And be on the complex phase ceramic and coarse particles refractory materials of representative with ZTA.But the report that utilizes the gel casting forming technology to prepare the BeO pottery is not seen as yet.
Summary of the invention
The objective of the invention is to propose a kind of method of the BeO of preparation pottery, be specifically related to utilize the gel casting forming technology to prepare the BeO pottery.Adopt the present invention to prepare the BeO pottery, raw material is handled simple, and operation is brief, the equipment less investment, and cost is low, and reduces operator and contact with the BeO powder, has reduced the murder by poisoning of BeO, suitable commercial scale production.
The objective of the invention is to realize in the following manner.
A kind of method of utilizing the gel casting forming technology to prepare the BeO pottery may further comprise the steps: the processing of BeO powder, BeO powder, sintering aid, organic monomer and linking agent, dispersion agent, deionized water mixed preparing gained mixing solutions after will handling carry out ball mill mixing, vacuum stripping, gel solidification, and the body drying binder removal after the gel solidification demoulding, sintering are promptly got the BeO pottery.
The processing of described BeO powder is earlier 600~1600 ℃ of calcinings 1~20 hour, then with the speed ball milling of 50~500rad/s 1~10 hour with the BeO powder.
The add-on of described organic monomer is 1%~30% of a BeO powder quality, and the part by weight of described organic monomer and linking agent is 1:1~50:1.
The add-on of described sintering aid is 0.01%~50% of a BeO powder quality; The add-on of described dispersion agent is 0.01%~10% of a BeO powder quality; The volume ratio of BeO powder and deionized water is 0.125~4.
Described mixing solutions pH value is 5~12.
Described sintering aid is SiO
2, Al
2O
3, MgO, Fe
2O
3, Y
2O
3, La
2O
3And Nd
2O
3In one or more; Organic monomer is a kind of in water miscible acrylamide or the Methacrylamide or both mixtures; Dispersion agent is an ammonium polyacrylate; Linking agent is N, N '-methylene-bisacrylamide.
Described mixing solutions was with the speed ball milling of 50~500rad/s 0.5~50 hour.
Carry out vacuum stripping after the described mixing solutions ball milling under whipped state, stirring velocity is 20~200rad/min, and vacuum tightness is 0.1~0.01Mpa, and the degasification time is 1~30 minute.
Add initiator and catalyzer after the described mixing solutions vacuum stripping, the back that stirs is injected mould and is solidified.
Described initiator is that concentration is 5%~10% ammonium persulfate aqueous solution; Catalyzer is a N,N,N.
Described dry binder removal was the base substrate after the demoulding to be dried to moisture earlier be not higher than 10%, and the speed with 0.5~5 ℃/min heats up in the time of 400~800 ℃ then, to temperature back insulation 0.5~3 hour; Be warming up to 1000~1500 ℃ with 10~30 ℃/min speed again, be incubated 1~5 hour.
Described sintering is that base substrate was carried out sintering 1~5 hour at 1500~2000 ℃.
Concrete technical scheme of the present invention is:
1, the processing of BeO powder
The powder loose density of the unit from China unique production BeO powder---Shuikoushan Mining Bureau's purchase is very low only to be 0.3g/cm
3About, granularity is very tiny, and water-absorbent is very strong, is not suitable for preparing ceramic size, therefore must calcine earlier, then ball-milling processing.Calcining temperature is 600~1600 ℃, and calcination time is 1~20 hour, and calcination atmosphere is vacuum or hydrogen atmosphere.Ball milling method is rolling ball milling, planetary ball mill or stirring ball-milling etc., and ball milling speed is 50~500rad/s, and the ball milling time is 1~10 hour.
2, batching
It is 5~12 solution that BeO powder, sintering aid, organic monomer and linking agent after will handling according to design requirements, dispersion agent, deionized water etc. are mixed with the pH value in proportion, with ammoniacal liquor or nitric acid adjust pH.Sintering aid is SiO
2, Al
2O
3, MgO, Fe
2O
3, Y
2O
3, La
2O
3And Nd
2O
3Deng in one or more.Organic monomer is one or more the mixture in water miscible acrylamide or the Methacrylamide; Linking agent is N, and N '-methylene-bisacrylamide, dispersion agent are ammonium polyacrylate; The add-on of organic monomer is 1%~30% of a BeO powder, and the part by weight of organic monomer and linking agent is 1:1~50:1.The add-on of sintering aid is 0.01%~50% of a BeO powder quality; The add-on of dispersion agent is 0.01%~10% of a BeO powder quality; The volume ratio of BeO powder and deionized water is 0.125~4.
3, ball mill mixing
The solution that configures is carried out ball milling.Ball milling speed is 50~500rad/s, and the ball milling time is 0.5~50 hour.
4, vacuum stripping
Slurry behind the ball milling is carried out vacuum stripping under whipped state, stirring velocity is 20~200rad/min, and vacuum tightness is 0.1~0.01Mpa, and the degasification time is 1~30 minute.
5, gel solidification
Add initiator and catalyzer in slurry, the back that stirs is injected preprepared grinding tool and is solidified.Initiator is that concentration is 5%~10% ammonium persulphate, and the add-on of ammonium persulphate is 0.1%~1% of an organic monomer weight; Catalyzer is N,N,N (TEMED), and add-on is 0.1%~1% of an organic monomer weight.The grinding tool material can be metal, glass, pottery, plastics etc.
6, dry binder removal
Base substrate after the demoulding is dry earlier, back binder removal.Drying mode has seasoning, blowing drying or heat drying etc., and the heat drying temperature is no more than 100 ℃, is dried to moisture and is lower than 10%.Binder removal speed is divided into and heats up at a slow speed and be rapidly heated: before 400~800 ℃, temperature rise rate is 0.5~5 ℃/min; Be warming up to 1000~1500 ℃ with 10~30 ℃/min speed again, be incubated 1~5 hour.
7, sintering
Base substrate is carried out sintering under air, vacuum or hydrogen atmosphere, sintering temperature is 1500~2000 ℃, and sintering time is 1~5 hour.
The present invention is scattered in the BeO ceramic powder in the aqueous solution that contains organic monomer and linking agent first, prepare the concentrated suspension of low viscosity and high solid volume fraction, add initiator then, suspensoid is injected mould, at certain temperature or adding catalyzer, cause the organic monomer polymerization, suspensoid viscosity increases severely, cause consolidation in-situ forming, obtain the very high base substrate of intensity through cryodrying.Proposed the concrete technical process and the technical scheme of the gel casting forming technology of suitable BeO pottery, and made it to satisfy the requirement of large-scale industrial production, its advantage is:
One, the gel casting forming technology is applied in the field of preparation BeO pottery, is easy to prepare the big part of BeO pottery, abnormal member etc.
Two, this method is that the wet moulding technology and the operation of ceramic body is brief, has reduced the time that operator contact with toxicity BeO powder.
Three, this method raw material is simple, cheap.
Four, this method industry mature and reliable is simple to operate, the production efficiency height.
Description of drawings
Fig. 1 prepares the process flow sheet of BeO pottery for the present invention;
Fig. 2 is for adopting the BeO ceramic sheet of the present invention's preparation;
Fig. 3 is for adopting the BeO ceramic bar of the present invention's preparation.
Embodiment
Below in conjunction with embodiment and embodiment the present invention is described in further detail.Primary BeO powder is slightly soluble in water, and loose density is very low, and this has influenced prepares high solids content, low viscous BeO ceramic size.The present invention adopts simple calcining ball-milling technology that the BeO powder is handled, and makes the BeO powder satisfy the requirement of preparation slurry, uses the gel casting forming technology to prepare the BeO stupalith then, and Fig. 1 is seen in concrete technical process.Main technique step of the present invention is as follows:
1, the processing of BeO powder
The powder loose density of the unit from China unique production BeO powder---Shuikoushan Mining Bureau's purchase is very low only to be 0.3g/cm
3About, granularity is very tiny, and water-absorbent is very strong, is not suitable for preparing ceramic size, therefore must calcine earlier, then ball-milling processing.Calcining temperature is 600~1600 ℃, and calcination time is 1~20 hour, and calcination atmosphere is vacuum or hydrogen atmosphere.Ball milling method is rolling ball milling, planetary ball mill or stirring ball-milling etc., and ball milling speed is 50~500rad/s, and the ball milling time is 1~10 hour.
2, batching
It is 5~12 solution that BeO powder, sintering aid, organic monomer and linking agent after will handling according to design requirements, dispersion agent, deionized water etc. are mixed with the pH value in proportion, with ammoniacal liquor or nitric acid adjust pH.Sintering aid is SiO
2, Al
2O
3, MgO, Fe
2O
3, Y
2O
3, La
2O
3And Nd
2O
3Deng in one or more.Organic monomer is one or more the mixture in water miscible acrylamide or the Methacrylamide; Linking agent is N, N '-methylene-bisacrylamide.The add-on of organic monomer is 1%~30% of a BeO powder, and the part by weight of organic monomer and linking agent is 1:1~50:1.The add-on of sintering aid is 0.01%~50% of a BeO powder quality; Dispersion agent is an ammonium polyacrylate, and add-on is 0.01%~10% of a BeO powder quality; The volume ratio of BeO powder and deionized water is 0.125~4.
3, ball mill mixing
The solution that configures is carried out ball milling.Ball milling speed is 50~500rad/s, and the ball milling time is 0.5~50 hour.
4, vacuum stripping
Slurry behind the ball milling is carried out vacuum stripping under whipped state, stirring velocity is 20~200rad/min, and vacuum tightness is 0.1~0.01Mpa, and the degasification time is 1~30 minute.
5, gel solidification
Add initiator and catalyzer in slurry, the back that stirs is injected preprepared grinding tool and is solidified.Initiator is that concentration is 5%~10% ammonium persulphate, and the add-on of ammonium persulphate is 0.1%~1% of an organic monomer weight; Catalyzer is N,N,N (TEMED), and add-on is 0.1%~1% of an organic monomer weight.The grinding tool material can be metal, glass, pottery, plastics etc.
6, dry binder removal
Base substrate after the demoulding is dry earlier, back binder removal.Drying mode has seasoning, blowing drying or heat drying etc., and the heat drying temperature is no more than 100 ℃, is dried to moisture and is lower than 10%.Binder removal technology was before 400~800 ℃, and temperature rise rate is 0.5~5 ℃/min, to temperature back insulation 0.5~3 hour; Rise to 1000~1500 ℃ with 10~30 ℃/min temperature rise rate then, be incubated 1~5 hour.
7, sintering
Base substrate is carried out sintering under air, vacuum or hydrogen atmosphere, sintering temperature is 1500~2000 ℃, and sintering time is 1~5 hour.
Embodiment 1
Prepare laminar BeO pottery
Take by weighing the 50gBeO powder and under 1200 ℃ of conditions, calcined 2 hours, then with the speed ball milling of 300rad/s 2 hours.With 50gBeO powder, 0.25gAl
2O
3Powder and 0.25gSiO
2Powder joins and contains the 4g acrylamide, and in the 15g deionized water of 1g methylene-bisacrylamide and 1g ammonium polyacrylate, adopting the nitre acid for adjusting pH value is 5; Ball mill mixing is 30 hours again.Carry out the vacuum stirring degasification after the discharging, stirring velocity is 20rad/min, and vacuum tightness is 0.1Mpa, and the time is 30min.Adding concentration is 10% ammonium persulfate solution 0.1ml and Tetramethyl Ethylene Diamine 0.05ml, after stirring, slurry is poured in the sheet glass mould that the slit is 1mm, places after 10 minutes, and pulp gel solidifies.Binder removal is carried out in wet base seasoning after the demoulding 48 hours then in air furnace, binder removal technology is with behind the temperature rise rate to 400 of 0.5 ℃/min ℃, is incubated 1 hour, with the temperature rise rate to 1200 of 30 ℃/min ℃, is incubated 1 hour again.Base substrate is put into vacuum oven carry out sintering, sintering temperature is 1800 ℃, and sintering time is 5 hours.Fig. 2 is for adopting the BeO ceramic sheet of this prepared.
Embodiment 2
Prepare shaft-like BeO pottery
Take by weighing the 100gBeO powder and under 1500 ℃ of conditions, calcined 4 hours, then with the speed ball milling of 500rad/s 1 hour.With 100gBeO powder, 0.5gAl
2O
3Powder, 0.25gSiO
2Powder and 0.25gY
2O
3Join and contain the 10g acrylamide, in the 20g deionized water of 2g methylene-bisacrylamide and 2g ammonium polyacrylate, adopting ammoniacal liquor to regulate the pH value is 12; Ball mill mixing is 20 hours again.Carry out the vacuum stirring degasification after the discharging, stirring velocity is 10rad/min, and vacuum tightness is 0.01Mpa, and the time is 10min.Adding concentration is 5% ammonium persulfate solution 1ml and Tetramethyl Ethylene Diamine 0.5ml, after stirring, slurry is poured in the metal circular hole assembling die that diameter is 1cm, places after 5 minutes, and pulp gel solidifies.Binder removal is carried out in wet base seasoning after the demoulding 24 hours then in air furnace, binder removal technology is with behind the temperature rise rate to 800 of 1 ℃/min ℃, is incubated 3 hours, with the temperature rise rate to 1300 of 20 ℃/min ℃, is incubated 2 hours again.Base substrate is put into vacuum oven carry out sintering, sintering temperature is 1700 ℃, and sintering time is 4 hours.Fig. 3 is for adopting the BeO ceramic bar of this prepared.
Embodiment 3
The optimization technical process one of preparation BeO pottery
Take by weighing the 100gBeO powder and under 600 ℃ of conditions, calcined 20 hours, then with the speed ball milling of 50rad/s 10 hours.With 100gBeO powder, 0.25gAl
2O
3Powder, 0.25gSiO
2Powder, 0.25g Fe
2O
3Powder and 0.25g La
2O
3Join and contain the 10g acrylamide, in the 20g deionized water of 10g methylene-bisacrylamide and 1g ammonium polyacrylate, adopting ammoniacal liquor condition pH value is 11; Ball mill mixing is 50 hours again.Carry out the vacuum stirring degasification after the discharging, stirring velocity is 10rad/min, and vacuum tightness is 0.01Mpa, and the time is 1min.Add concentration and be 10% ammonium persulfate solution 1ml and Tetramethyl Ethylene Diamine 0.1ml, after stirring, slurry is poured in the prior ready assembling die, leave standstill 30 minutes after, pulp gel solidifies.Binder removal is carried out in wet base seasoning after the demoulding 48 hours then in air furnace, binder removal technology is with behind the temperature rise rate to 600 of 0.5 ℃/min ℃, is incubated 3 hours, with the temperature rise rate to 1000 of 10 ℃/min ℃, is incubated 5 hours again.Base substrate is put into vacuum oven carry out sintering, sintering temperature is 1500 ℃, and sintering time is 5 hours.
Embodiment 4
The optimization technical process two of preparation BeO ceramic bar
Take by weighing the 100gBeO powder and under 1600 ℃ of conditions, calcined 1 hour, then with the speed ball milling of 500rad/s 1 hour.With 100gBeO powder, 0.5gAl
2O
3Powder, 0.2gLa
2O
3Powder and 0.3gNd
2O
3Powder joins and contains the 25g acrylamide, and in the 20g deionized water of 10g methylene-bisacrylamide and 0.5g ammonium polyacrylate, adopting ammoniacal liquor to regulate the pH value is 8; Ball mill mixing is 20 hours again.Carry out the vacuum stirring degasification after the discharging, stirring velocity is 200rad/min, and vacuum tightness is 0.01Mpa, and the time is 30min.Adding concentration is 5% ammonium persulfate solution 2ml and Tetramethyl Ethylene Diamine 1ml, after stirring, slurry is poured in the circular hole assembling die that diameter is 1cm, places after 1 minute, and pulp gel solidifies.Binder removal is carried out in wet base seasoning after the demoulding 48 hours then in air furnace, binder removal technology is with behind the temperature rise rate to 800 of 5 ℃/min ℃, is incubated 0.5 hour, with the temperature rise rate to 1300 of 10 ℃/min ℃, is incubated 2 hours again.Base substrate is put into vacuum oven carry out sintering, sintering temperature is 2000 ℃, and sintering time is 1 hour.
Embodiment 5
The optimization technical process three of preparation BeO ceramic bar
Take by weighing the 50gBeO powder and under 600 ℃ of conditions, calcined 1 hour, then with the speed ball milling of 50rad/s 1 hour.With 50gBeO powder, 0.25gAl
2O
3Powder, 0.25gSiO
2Powder, 0.2gLa
2O
3Powder, 0.1gNd
2O
3Powder and 0.2gY
2O
3Join and contain the 10g acrylamide, in the 20g deionized water of 2g methylene-bisacrylamide and 2g ammonium polyacrylate, adopting the nitre acid for adjusting pH value is 6; Ball mill mixing is 20 hours again.Carry out the vacuum stirring degasification after the discharging, stirring velocity is 10rad/min, and vacuum tightness is 0.1Mpa, and the time is 30min.Adding concentration is 10% ammonium persulfate solution 1ml and Tetramethyl Ethylene Diamine 1ml, after stirring, slurry is poured in the metal die, places about 20 minutes, and pulp gel solidifies.Binder removal is carried out in wet base seasoning after the demoulding 48 hours then in air furnace, binder removal technology is with behind the temperature rise rate to 400 of 0.5 ℃/min ℃, is incubated 3 hours, with the temperature rise rate to 1300 of 10 ℃/min ℃, is incubated 2 hours again.Base substrate is put into vacuum oven carry out sintering, sintering temperature is 1500 ℃, and sintering time is 4 hours.
Claims (12)
1, a kind of method of utilizing the gel casting forming technology to prepare the BeO pottery, it is characterized in that may further comprise the steps: the processing of BeO powder, BeO powder, sintering aid, organic monomer and linking agent, dispersion agent, deionized water mixed preparing gained mixing solutions after will handling carry out ball mill mixing, vacuum stripping, gel solidification, and the body drying binder removal after the gel solidification demoulding, sintering are promptly got the BeO pottery.
2, the method for utilizing the gel casting forming technology to prepare the BeO pottery according to claim 1, it is characterized in that, the processing of described BeO powder is earlier 600~1600 ℃ of calcinings 1~20 hour, then with the speed ball milling of 50~500rad/s 1~10 hour with the BeO powder.
3, the method for utilizing the gel casting forming technology to prepare the BeO pottery according to claim 1, it is characterized in that, the add-on of described organic monomer is 1%~30% of a BeO powder quality, and the part by weight of described organic monomer and linking agent is 1:1~50:1.
4, the method for utilizing the gel casting forming technology to prepare the BeO pottery according to claim 1 is characterized in that, the add-on of described sintering aid is 0.01%~50% of a BeO powder quality; The add-on of described dispersion agent is 0.01%~10% of a BeO powder quality; The volume ratio of BeO powder and deionized water is 0.125~4.
5, the method for utilizing the gel casting forming technology to prepare the BeO pottery according to claim 1 is characterized in that, described mixing solutions pH value is 5~12.
6, according to claim 1 or the 3 or 4 described methods of utilizing the gel casting forming technology to prepare the BeO pottery, it is characterized in that described sintering aid is SiO
2, Al
2O
3, MgO, Fe
2O
3, Y
2O
3, La
2O
3And Nd
2O
3In one or more; Organic monomer is a kind of in water miscible acrylamide or the Methacrylamide or both mixtures; Dispersion agent is an ammonium polyacrylate; Linking agent is N, N '-methylene-bisacrylamide.
7, the method for utilizing the gel casting forming technology to prepare the BeO pottery according to claim 1 is characterized in that, described mixing solutions was with the speed ball milling of 50~500rad/s 0.5~50 hour.
8, the method for utilizing the gel casting forming technology to prepare the BeO pottery according to claim 1, it is characterized in that, under whipped state, carry out vacuum stripping after the described mixing solutions ball milling, stirring velocity is 20~200rad/min, vacuum tightness is 0.1~0.01Mpa, and the degasification time is 1~30 minute.
9, the method for utilizing the gel casting forming technology to prepare the BeO pottery according to claim 1 is characterized in that, adds initiator and catalyzer after the described mixing solutions vacuum stripping, and the back that stirs is injected mould and solidified.
10, the method for utilizing the gel casting forming technology to prepare the BeO pottery according to claim 9 is characterized in that, described initiator is that concentration is 5%~10% ammonium persulfate aqueous solution; Catalyzer is a N,N,N.
11, the method for utilizing the gel casting forming technology to prepare the BeO pottery according to claim 1, it is characterized in that, described dry binder removal is the base substrate after the demoulding to be dried to moisture earlier be not higher than 10%, speed with 0.5~5 ℃/min heated up in the time of 400~800 ℃ then, to temperature back insulation 0.5~3 hour; Be warming up to 1000~1500 ℃ with 10~30 ℃/min speed again, be incubated 1~5 hour.
12, the method for utilizing the gel casting forming technology to prepare the BeO pottery according to claim 1 is characterized in that, described sintering is that base substrate was carried out sintering 1~5 hour at 1500~2000 ℃.
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